Phenyl Isothiocyanate → HCID 54237642、化合物

HRID 647584ノート

反応式

HRID 647584 の反応式
C[O-].[Na+].I.[NH:5]=[C:6]1[N:10]([CH3:11])[CH:9]=[CH:8][S:7]1.[C:12]1([N:18]=[C:19]=[S:20])[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1>C(O)C.C1(C)C=CC=CC=1>[CH3:11][N:10]1[CH:9]=[CH:8][S:7][C:6]1=[N:5][C:19]([NH:18][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)=[S:20]

参加物

6

反応物 3

HCID 7673Phenyl IsothiocyanateHCID 10942334Sodium MethoxideHCID 429153603-METHYL-1,3-THIAZOL-2(3H)-IMINE HYDROIODIDE

生成物 1

HCID 54237642HCID 54237642、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 1140Toluene溶媒

実験手順

Sodium methoxide (5.40 g) was added to a stirred mixture of 2-imino-3-methylthiazoline hydroiodide (24.95 g) in ethanol (100 ml) and the mixture brought to reflux. Phenyl isothiocyanate (16.35 g) in toluene (50 ml) was added over 30 minutes and reflux continued for a further hour then cooled in ice. The solid obtained on filtration and washing with ethanol and water was dried to give the product, mpt 172.5°-173.5°. Recrystallisation from iso-propanol gave analytically pure product, mpt 173.5°-174°.

後処理

  1. temperatureto reflux
  2. temperaturereflux
  3. waitcontinued for a further hour
  4. temperaturethen cooled in ice
  5. customThe solid obtained on filtration
  6. washwashing with ethanol and water
  7. customwas dried
  8. customto give the product, mpt 172.5°-173.5°
  9. customRecrystallisation from iso-propanol
  10. customgave analytically pure product, mpt 173.5°-174°

出典と根拠

ORDレコード
ord-2dd75946f83a4ef09305d7039efdd6e7
出典データセット
uspto-grants-1983_10
特許番号
US04409216

反応ノート

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